Method for detecting residues of eight organic matters in ion exchange resin by adopting headspace gas phase method
A technology of ion exchange resin and headspace gas phase, applied in the field of chemical analysis, to achieve the effect of optimizing chromatographic conditions, good separation, and improving accuracy
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Embodiment 1
[0061] (1) Preparation of standard working solution:
[0062] Prepare standard working solution of methyl isopropyl ketone: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0063] Prepare standard working solution of methyl methacrylate: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0064] Prepare 3-pentanone standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200 μg / mL,
[0065] Prepare standard working solution of methyl butyrate: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0066] Prepare 1,2-dichloroethane standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0067] Prepare 1,3-diethylbenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0068] Prepare 1,4-diethylbenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,
[0069] Prepare m-dichlorobenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL; the solvents are dimethyl sulfoxide stand...
Embodiment 2
[0090] (1) Optimization of headspace sampler equilibrium temperature:
[0091] On the basis of Example 1, under the condition of other parameters being fixed, samples were injected after equilibrating at constant temperature of 50, 60, 70, and 80°C in the headspace for 30 minutes, and the influence of different equilibrium temperatures on the peak area of the target was investigated.
[0092] See Figure 15 ~ Figure 18 . The results show that in the range of 40-90°C, the peak areas of the eight organic compounds increase with the increase of temperature, and the analysis sensitivity is higher; Condensation, resulting in reduced accuracy and possibly increased interference. Combined with the constant temperature state control performance of the sampler, headspace pressure resistance and tightness and other factors, 80°C was selected as the standard equilibrium temperature.
[0093] (2) Optimization of headspace sampler equilibration time:
[0094] On the basis of Example ...
Embodiment 3
[0097] (1) Selection of chromatographic column:
[0098] When using DB-624 (30m×0.53mm, 1.0μm) quartz capillary column and DB-WAX (30m×0.25mm×0.25μm) quartz capillary column to separate the mixed standard, the 8 kinds of organic substances could not be separated, see Figure 22 ~ Figure 24 , it can be seen that the separation effect of the sample is good when using DB-23 (30m×0.25mm×0.25μm).
[0099] (2) The solvent is replaced by methanol: see the peak results when methanol is used as the solvent Figure 25 , may overlap with the target organism and result in inaccurate results.
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